CN1040559A - The manufacture method of alpha-silicon nitride powders and equipment - Google Patents
The manufacture method of alpha-silicon nitride powders and equipment Download PDFInfo
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- CN1040559A CN1040559A CN 89106804 CN89106804A CN1040559A CN 1040559 A CN1040559 A CN 1040559A CN 89106804 CN89106804 CN 89106804 CN 89106804 A CN89106804 A CN 89106804A CN 1040559 A CN1040559 A CN 1040559A
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- liquefied ammonia
- silicon
- organic solvent
- imide
- silicon imide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/068—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with silicon
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Abstract
A kind of equipment of manufacture method of alpha-silicon nitride powders, method of the present invention is to use SiCl
4With the liquefied ammonia generation silicon imide that on the organic solvent interface, reacts, be heated then to decompose and make Si
3N
4Powder.Realize continuous charging by equipment such as reactor, spray scrubber, wet cyclone, thermolysis crystallization rotary kilns, discharging reaches continuous production Si continuously
3N
4The purpose of powder.High-purity, the ultra-fine Si of the product that method of the present invention obtained
3N
4α-Si in the powder
3N
4＞96%, 0＜1%, C＜10PPM, Cl
-＜10PPM, metal total impurities content＜300PPM, granularity＜0.5 μ m, productive rate reaches 97%.
Description
The present invention relates to a kind of manufacture method and equipment of alpha-silicon nitride powders, be applicable to the preparation of metal nitride, product is used to prepare the nitride goods with superhard resistance toheat.It comprises the steps: that at first silicon tetrachloride and liquefied ammonia generate silicon imide in the organic solvent surface reaction, then the silicon imide thermolysis is made alpha-silicon nitride powders.
Disclose a kind of metal silicon nitride manufacturing method of power in the clear 56-44006 of Japanese Patent, its purpose is in order to solve remove and problem by product halogeno-amine " smog " occluding device, pipeline of the reaction heat that metal halide and liquefied ammonia vigorous reaction are produced in the prior art.Its content be in the reactor of liquefied ammonia and metal halide adding immiscible with it and organic solvent that proportion is bigger than liquefied ammonia, the reaction of metal halide and liquefied ammonia can carry out the reaction that generates silicon imide by realizing in the organic solvent layer that metal halide is passed into the reaction system bottom smoothly.Its weak point is that this method is a step reaction, can not serialization production, after every batch reaction is finished, need all shift away solvent and product, solvent load is very big, silicon imide being transferred in the electric furnace in the pyrolysated process, cause the oxygen level of product to raise in addition also easily by aquation, oxidation, organic solvent with separating of product the bad carbon content of product that also causes easily increase.
The objective of the invention is to avoid above-mentioned weak point of the prior art and a kind of manufacturing high pure and ultra-fine Si is provided
3N
4The continuous production method of powder reaches the C, the Cl that reduce in the product simultaneously
-With the purpose of 0 foreign matter content such as grade, improve Si
3N
4The quality of powder reduces the consumption of organic solvent.
Purpose of the present invention can reach by following measure:
The present invention generates silicon imide with silicon tetrachloride and liquefied ammonia in the organic solvent surface reaction, is heated then and decomposes the method and apparatus that makes alpha-silicon nitride powders, it is characterized in that carrying out continuously as follows:
(a) silicon imide is synthetic: at first add liquefied ammonia and the immiscible with it and proportion organic solvent greater than liquefied ammonia in the reactor that agitator and multihole distributor are housed [2], feed in the organic solvent layer continuously tetrazotization silicon and rare gas element and constantly additional liquefied ammonia then, rare gas element carries silicon tetrachloride and evenly arrives organic solvent and liquefied ammonia interface by multihole distributor [8a], generate silicon imide and ammonium chloride with the liquefied ammonia reaction, float on above the organic solvent layer, reaction heat is absorbed as heat of gasification by liquefied ammonia and makes the gasification of part liquefied ammonia, the NH of generation
4Cl smog is also absorbed by liquefied ammonia, avoids pipe-line equipment to stop up, and reaction can continuously be carried out.
(b) washing of silicon imide: silicon imide that generates in reactor and byproduct ammonia chloride are flowed through by reactor outlet with the liquefied ammonia fluid spray scrubber [3] of liquefied ammonia nozzle [10] and porous filter plate [8b] are housed, in spray scrubber, silicon imide obtains washing, by product NH
4Cl is dissolved in the liquefied ammonia, by reclaiming behind the porous filter plate.The spray rate of liquefied ammonia can be regulated according to the speed that reaction is carried out, and guarantees the silicon imide washing fully.
(c) solid-liquid separation: the silicon imide after the spray scrubber washing flows into wet cyclone [4] with the liquefied ammonia fluid by the spray scrubber outlet, separates through spinning liquid, and silicon imide separates with liquefied ammonia, the liquefied ammonia recycling use, and silicon imide enters thermal decomposition furnace.
(d) thermolysis: the silicon imide from wet cyclone enters thermolysis crystallization processing stove [5] continuously, heats in inert gas atmosphere, successively enters arid zones, thermolysis band and crystallization band, makes α-Si at last
3N
4Powder, discharging continuously.
Purpose of the present invention can also reach by following concrete measure:
The organic solvent that silicon tetrachloride and liquefied ammonia reaction generate the required usefulness of silicon imide is aliphatic hydrocarbon or the aromatic hydrocarbon that contains 5～7 carbon atoms in the molecule, or any two or more mixture wherein, toluene is adopted in suggestion: hexanaphthene=1: 1, according to method of the present invention, organic solvent once adds and can use continuously, in the batch synthesis method described in the Japanese Patent JP5644006, every production 1 gram Si
3N
4Powder need consume the 33ml organic solvent.
Synthetic and the thermolysis of silicon imide all need be carried out in inert gas atmosphere, and nitrogen is adopted in suggestion.
The raw material silicon tetrachloride and the liquefied ammonia of synthetic silicon imide will feed in accordance with the appropriate ratio, and the ratio that suggestion is adopted is SiCl
4: NH
3=1: 10～20, preferably adopt 1: 10～15, can guarantee the SiCl that feeds like this
4Complete reaction can make reaction heat in time take away by product NH again
4Cl " smog " also can fully be absorbed, and guarantees the carrying out that reaction is continual and steady.
Multihole distributor in multihole distributor in the reactor [2] and the spray thrower [3] is made the most handy porous ceramic plate by metal, plastics, stupalith.
The installation site of multihole distributor [8a] is apart from reactor outlet lower edge 5～20cm, 3cm at least.The effect of this grid distributor is to make raw material SiCl
4Be diffused on the interface equably and react, simultaneously product and organic solvent are played buffer action, the silicon imide of generation is accumulated on grid distributor, surpass outlet and make in the inflow spray scrubber.
The building-up reactions of silicon imide can be carried out under atmospheric low-temperature, also can add to depress at normal temperature and carry out, and considers that our suggestion of equipment manufacturing cost carries out under atmospheric low-temperature, and the temperature of reaction that suggestion is adopted is 0～-80 ℃, preferably-40～-55 ℃.
The main filtration of the screen plate of spray scrubber bottom, its setting angle α is 45 °～80 °, is preferably in 60 °～75 °.Product C l after the washing
-Content is lower than 10PPM.
It is that continuous analysing silicon imines is made α-Si that the thermolysis crystallization is handled stove [5]
3N
4Key equipment, preferably adopt the rotary type stove and tilt to install, along with the rotation of tilting rotary kiln, silicon imide enters arid zones, thermolysis band and crystallization band in proper order, finally can obtain high-purity ultra-fine a-Si continuously
3N
4Powder.
The most outstanding feature of method of the present invention is by equipment continuously feeding of the present invention, and discharging has continuously realized Si
3N
4The serialization of powder production, thus the productive rate and the quality of product improved.
The related key equipment of method of the present invention is the reactor of band stirring and multihole distributor, spray-type washer, wet cyclone and tilting rotary furnace.
The drawing of accompanying drawing is described as follows:
Fig. 1, manufacturing Si
3N
4The processing unit synoptic diagram of powder.
1 anhydrous ammonia tank, 2 reactors, 3 spray scrubbers, 4 wet cyclones, 5 thermolysis crystallizations are handled stove, 6 liquefied ammonia, NH
4Cl withdrawing can, 7 thermolysis crystallization stove seal casinghousings, 8a multihole distributor, 8b porous filter plate, 9 agitators, 10 spray washing shower nozzles, 11a liquefied ammonia valve, 11b liquefied ammonia valve, 12N
2Air valve, 13SiCl
4, organic solvent adds valve, 14, blow-off valve, 15 vacuum valves, 16 reactor outlet valves, 17 liquefied ammonia fluid valves, 18N
2Air valve, 19 α-Si
3N
4Liquefied ammonia, NH after bleeder valve, 20 washings
4Cl recovery valve, 21 liquefied ammonia gasification recovery valve, 22 by product NH
4The Cl bleeder valve.
Fig. 2, X-diffractogram.
Fig. 3, stereoscan photograph.
The present invention will now be further detailed embodiment:
Embodiment 1:
Adopt fluorine Lyons or dry ice refrigeration means that reactor [2] is cooled to-50 ℃, the empty footpath of porous ceramics grid distributor is 1mm, and pore size distribution is 25 hole/inches, and grid distributor is from outlet lower edge 10cm.Shut-off valve [19], [20], [17], [18], [11a], [11b], [13], [12], [14], open valve [16], [15] vacuumize half an hour, shut-off valve [15] is then opened the logical N of valve [12]
2, three times so repeatedly, make total system become N
2Atmosphere.Shut-off valve [15], [16], [12] are opened [13] and added toluene: the mixed organic solvents of hexanaphthene=1: 1 is to 7cm place, porous plate pottery grid distributor upper end, and shut-off valve [13] is opened valve [11a] and put into liquefied ammonia to 30cm place, discharge port upper edge, opens valve [12] and leads to N
2Bubbling is opened valve [13] and is fed SiCl
4To reactor bottom, start agitator [9] simultaneously, SiCl
4Be diffused in the organic solvent, along with N
2Bubble agitate stirring with agitator, the SiCl in the solvent
4Upwards be diffused into interfacial layer equably by porous ceramics grid distributor [8a] and contact with liquefied ammonia and react, open valve [16], the silicon imide of generation flows in the spray scrubber [3] with the liquefied ammonia fluid, by product NH
4The Cl major part is dissolved in the liquefied ammonia liquid, and reaction generates heat and makes the gasification of part liquefied ammonia.So adjust SiCl
4And NH
3Throughput ratio at 10ml/min: 100ml/min, control mixing speed be 300 rev/mins, N
2The amount of blasting be 3l/min, make the reaction continual carrying out.Open valve [11b] and enable spray scrubber [3], liquefied ammonia makes the NH in the silicon imide by the silicon imide that the drip washing of spray scrubber nozzle generates
4Cl dissolves by the drip washing repeatedly of liquefied ammonia and is filled in the withdrawing can [6] by filter plate of porous ceramic [8b] with liquefied ammonia, silicon imide flows in the wet cyclone [4] after washing, separate through spinning liquid, liquid phase flows in the withdrawing can [6], the solid product silicon imide flows in the rotary kiln [5], opens the logical N of valve [8]
2, silicon imide is through 100～600 ℃ of dryings in low temperate zone, and 600～1200 ℃ of thermolysiss in temperate zone in entering enter 1200～1550 ℃ on crystallization band at last, begin after 5 hours to utilize the storage in vacuum mode to collect the Si of generation from discharge port [19]
3N
4Powder.The final product that generates is a white powder, through X-diffraction analysis α-Si
3N
4Content is 96%, β-Si
3N
4Be 4%, [Fig. 2]; The scanning electron microscope analysis product is for there being the spheroidal particle [Fig. 3] of reunion slightly, and sreen analysis shows; Particle＜0.5 μ m; Chemical analysis shows 0＜1%, Cl
-＜10PPM, C＜10PPM, metal total impurities content Me＜300PPM.Productive rate reaches 97%.
Embodiment 2:
With embodiment 1 identical operation steps and order, with the temperature regulation to 0 of reactor ℃, organic solvent is selected hexanaphthene for use, and the pressure of keeping reactor is 4.5kg/cm
2, the angle [alpha] of regulating spray scrubber [3] is 70 ℃, the product that obtains at last is α-Si
3N
4Powder, performance, purity are identical with embodiment 1, and productive rate is 81%.
The present invention has following advantage than prior art:
1, can produce continuously.
2, organic solvent once adds, the long-term use.
3, improve the quality of products 0＜1%, Cl-＜10PPM, C＜10PPM, metal total impurities content＜300PPM.
4, improving productive rate reaches more than 97%.
Claims (11)
1, a kind of silicon tetrachloride and liquefied ammonia used generates silicon imide in the organic solvent surface reaction, is heated then and decomposes the method and apparatus that makes alpha-silicon nitride powders, it is characterized in that carrying out continuously as follows:
(a) silicon imide is synthetic: at first add liquefied ammonia and the immiscible with it and proportion organic solvent greater than liquefied ammonia in the reactor that agitator and multihole distributor are housed [2], feed in the organic solvent layer continuously tetrazotization silicon and rare gas element and constantly additional liquefied ammonia then, rare gas element carries silicon tetrachloride and evenly arrives organic solvent and liquefied ammonia interface by multihole distributor [8a], generate silicon imide and by-product ammonium chloride with the liquefied ammonia reaction, float on above the organic solvent.
(b) washing of silicon imide: the silicon imide of generation and byproduct ammonia chloride are flowed through by reactor outlet with the liquefied ammonia fluid spray scrubber [3] of liquefied ammonia nozzle [10] and porous filter plate [8b] are housed, silicon imide obtains washing, and the by product ammonia chloride is dissolved in the liquefied ammonia by reclaiming behind the porous filter plate.
(c) solid-liquid separation: the silicon imide after the washing flows into wet cyclone [4] with the liquefied ammonia fluid by the spray scrubber outlet, separates through spinning liquid, and silicon imide separates with liquefied ammonia.
(d) thermolysis: silicon imide enters the thermolysis crystallization continuously and handles stove [5], thermal degradation and carry out crystallization and make α-Si in inert gas atmosphere
3N
4Powder.
2, according to claim 1, it is characterized in that the organic solvent described in (a) is to contain the aliphatic hydrocarbon of 5～7 carbon atoms or aromatic hydrocarbon or two or more mixture arbitrarily wherein in the molecule, toluene is adopted in suggestion: hexanaphthene=1: 1.
3, according to claim 1, it is characterized in that (a) and (d) described in rare gas element nitrogen preferably.
4,, it is characterized in that reactant liquefied ammonia and the SiCl described in (a) according to claim 1
4The feeding ratio be SiCl
4: NH
3=1: 10～15.
5, according to claim 1, it is characterized in that the multihole distributor described in (a) [8a] and (b) described in multihole distributor [8b] make the most handy porous ceramic plate by metal, plastics, stupalith.
6, according to claim 1, the installation site that it is characterized in that the multihole distributor described in (a) is apart from reactor outlet lower edge 5～20cm, 3cm at least.
7, according to claim 1, it is characterized in that the building-up reactions of the silicon imide described in (a) can be carried out under atmospheric low-temperature, also can add to depress and carry out at normal temperature, the temperature of reaction that suggestion is adopted is 0～-80 ℃, preferably-40～-55 ℃ between.
8, according to claim 1, the setting angle α that it is characterized in that the screen plate of the spray scrubber bottom described in (b) is 45 °～80 °, best 60 °～75 °.
9,, it is characterized in that it is the rotary type stove that (d) described thermolysis crystallization is handled stove according to claim 1.
10,, it is characterized in that described method by described equipment continuously feeding, discharging continuously according to claim 1.
11, according to the related equipment of the described method of claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89106804 CN1013659B (en) | 1989-08-24 | 1989-08-24 | Method and facility for producing silicon nitride powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89106804 CN1013659B (en) | 1989-08-24 | 1989-08-24 | Method and facility for producing silicon nitride powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1040559A true CN1040559A (en) | 1990-03-21 |
| CN1013659B CN1013659B (en) | 1991-08-28 |
Family
ID=4856878
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 89106804 Expired CN1013659B (en) | 1989-08-24 | 1989-08-24 | Method and facility for producing silicon nitride powder |
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| Country | Link |
|---|---|
| CN (1) | CN1013659B (en) |
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0410107A2 (en) * | 1989-07-22 | 1991-01-30 | Hüls Aktiengesellschaft | Process for the preparation of silicon dimide with a low carbon content |
| CN1064024C (en) * | 1997-11-20 | 2001-04-04 | 浙江大学 | Method and apparatus for production of high purity ultrafine silicon nitride |
| CN104925764A (en) * | 2015-06-12 | 2015-09-23 | 常州汉耀复合材料有限公司 | Novel device for generating silicone imine continuously |
| CN105217583A (en) * | 2015-09-28 | 2016-01-06 | 韩召 | A kind of method preparing nano level high purity silicon nitride |
| CN106367733A (en) * | 2015-07-24 | 2017-02-01 | 东莞市中镓半导体科技有限公司 | Apparatus and method for removing tail gas deposits in HVPE device pipeline |
| CN106672922A (en) * | 2015-11-11 | 2017-05-17 | 新特能源股份有限公司 | System for producing silicon nitride |
| CN107557866A (en) * | 2017-08-28 | 2018-01-09 | 青岛桥海陶瓷新材料科技有限公司 | The preparation method of silicon nitride crystal whisker |
| CN107954723A (en) * | 2017-12-19 | 2018-04-24 | 清华大学 | A kind of preparation method of α phase silicon nitride powders |
| CN108394876A (en) * | 2017-02-07 | 2018-08-14 | 新疆晶硕新材料有限公司 | Nitrogen silane and its production method, silicon nitride and its production method |
| CN108928806A (en) * | 2017-05-25 | 2018-12-04 | 新疆晶硕新材料有限公司 | A kind of method and silicon imide synthesizing silicon imide |
| CN109384206A (en) * | 2017-08-09 | 2019-02-26 | 新疆晶硕新材料有限公司 | The production system and production method of the process units and production method of silicon imide, silicon nitride |
| CN109608205A (en) * | 2019-02-02 | 2019-04-12 | 清华大学 | A method of the shaft-like α phase silicon nitride powder such as preparing |
| CN113148966A (en) * | 2021-04-20 | 2021-07-23 | 安徽工业大学 | Method for preparing high-purity silicon nitride powder by ammonolysis method |
| CN113614034A (en) * | 2019-03-29 | 2021-11-05 | 电化株式会社 | Silicon nitride powder, method for producing same, and method for producing silicon nitride sintered body |
| CN115106031A (en) * | 2022-05-21 | 2022-09-27 | 倪磊 | Fluorine-silicon separation equipment for fluorine-silicon mixture |
| WO2024045103A1 (en) * | 2022-08-31 | 2024-03-07 | 南京延长反应技术研究院有限公司 | Reaction system and method for producing silicon nitride |
-
1989
- 1989-08-24 CN CN 89106804 patent/CN1013659B/en not_active Expired
Cited By (24)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0410107A2 (en) * | 1989-07-22 | 1991-01-30 | Hüls Aktiengesellschaft | Process for the preparation of silicon dimide with a low carbon content |
| CN1064024C (en) * | 1997-11-20 | 2001-04-04 | 浙江大学 | Method and apparatus for production of high purity ultrafine silicon nitride |
| CN104925764A (en) * | 2015-06-12 | 2015-09-23 | 常州汉耀复合材料有限公司 | Novel device for generating silicone imine continuously |
| CN106367733B (en) * | 2015-07-24 | 2019-02-22 | 东莞市中镓半导体科技有限公司 | A kind of device and method for removing HVPE equipment pipe tail gas deposit |
| CN106367733A (en) * | 2015-07-24 | 2017-02-01 | 东莞市中镓半导体科技有限公司 | Apparatus and method for removing tail gas deposits in HVPE device pipeline |
| CN105217583B (en) * | 2015-09-28 | 2017-05-31 | 青岛桥海陶瓷新材料科技有限公司 | A kind of method for preparing nanoscale high purity silicon nitride |
| CN105217583A (en) * | 2015-09-28 | 2016-01-06 | 韩召 | A kind of method preparing nano level high purity silicon nitride |
| CN106672922B (en) * | 2015-11-11 | 2019-01-22 | 新疆晶硕新材料有限公司 | A kind of system producing silicon nitride |
| CN106672922A (en) * | 2015-11-11 | 2017-05-17 | 新特能源股份有限公司 | System for producing silicon nitride |
| CN108394876A (en) * | 2017-02-07 | 2018-08-14 | 新疆晶硕新材料有限公司 | Nitrogen silane and its production method, silicon nitride and its production method |
| CN108928806A (en) * | 2017-05-25 | 2018-12-04 | 新疆晶硕新材料有限公司 | A kind of method and silicon imide synthesizing silicon imide |
| CN108928806B (en) * | 2017-05-25 | 2020-08-04 | 新疆晶硕新材料有限公司 | Method for synthesizing silicon imine and silicon imine |
| CN109384206A (en) * | 2017-08-09 | 2019-02-26 | 新疆晶硕新材料有限公司 | The production system and production method of the process units and production method of silicon imide, silicon nitride |
| CN109384206B (en) * | 2017-08-09 | 2020-07-17 | 新疆晶硕新材料有限公司 | Production device and production method of silicon imine, production system and production method of silicon nitride |
| CN107557866A (en) * | 2017-08-28 | 2018-01-09 | 青岛桥海陶瓷新材料科技有限公司 | The preparation method of silicon nitride crystal whisker |
| CN107954723B (en) * | 2017-12-19 | 2020-11-10 | 清华大学 | Preparation method of alpha-phase silicon nitride powder |
| CN107954723A (en) * | 2017-12-19 | 2018-04-24 | 清华大学 | A kind of preparation method of α phase silicon nitride powders |
| CN109608205A (en) * | 2019-02-02 | 2019-04-12 | 清华大学 | A method of the shaft-like α phase silicon nitride powder such as preparing |
| CN109608205B (en) * | 2019-02-02 | 2021-04-16 | 清华大学 | Method for preparing equiaxed alpha-phase silicon nitride powder |
| CN113614034A (en) * | 2019-03-29 | 2021-11-05 | 电化株式会社 | Silicon nitride powder, method for producing same, and method for producing silicon nitride sintered body |
| CN113148966A (en) * | 2021-04-20 | 2021-07-23 | 安徽工业大学 | Method for preparing high-purity silicon nitride powder by ammonolysis method |
| CN113148966B (en) * | 2021-04-20 | 2022-04-29 | 安徽工业大学 | Method for preparing high-purity silicon nitride powder by ammonolysis method |
| CN115106031A (en) * | 2022-05-21 | 2022-09-27 | 倪磊 | Fluorine-silicon separation equipment for fluorine-silicon mixture |
| WO2024045103A1 (en) * | 2022-08-31 | 2024-03-07 | 南京延长反应技术研究院有限公司 | Reaction system and method for producing silicon nitride |
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|---|---|
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